HRID1468692
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 7-bromo-2-cyclopropyl-5-methylbenzo[d]thiazol-6-yl trifluoromethanesulfonate (16) (410 mg, 0.988 mmol) in DMF (4 ml), was added tributylvinyltin (0.43 ml, 1.47 mmol), LiCl (125 mg, 2.94 mmol) and PdCl2(PPh3)2 (70 mg, 0.096 mmol). The reaction mixture was reacted at 80° C. overnight. The reaction was cooled down, washed by saturated NaHCO3 solution, extracted by EtOAc. The organic phase was combined, dry over MgSO4, filtered, concentrated and purified by silica gel column, eluting by 0-50% EtOAc in hexanes.
WORKUP
后处理
- customThe reaction mixture was reacted at 80° C. overnight
- temperatureThe reaction was cooled down
- washwashed by saturated NaHCO3 solution
- extractionextracted by EtOAc
- dry with materialdry over MgSO4
- filtrationfiltered
- concentrationconcentrated
- custompurified by silica gel column
- washeluting by 0-50% EtOAc in hexanes